KR101304996B1 - Synthesis of SiAlON Phosphors by Flux Addition - Google Patents

Abstract

A method for producing alpha sialon phosphor powder having a uniform particle size and good luminance characteristics is disclosed. The present invention, in the method for producing α-SiAlON phosphor represented by M1xM2ySi12-m-nAlm + nOnN16-n, preparing a starting material comprising silicon nitride, aluminum nitride, the compound of the M1, M2 metal in a predetermined ratio ; Mixing 5-10% by weight of non-metal fluoride or non-metal chloride with a weight ratio of the starting material composition; And firing the mixture provides a method for producing α-SiAlON phosphor comprising the step of synthesizing α-SiAlON. According to the present invention, it is possible to provide a method for producing a nitride phosphor whose particle shape, size and surface defects can be controlled even by low energy grinding after synthesis.

Description

Synthesis method of sialon phosphor powder using flux {Synthesis of SiAlON Phosphors by Flux Addition}

The present invention relates to a method for synthesizing sialon phosphor powder, and more particularly, to a method for producing alpha sialon phosphor powder having a uniform particle size and good brightness characteristics with controlled particle shape.

There are many ways to realize white light in an LED device, but the most typical method is a blue LED light emitting chip and a yellow phosphor excited by the blue LED light emitting chip. Such an implementation method has been developed by combining a blue LED light emitting chip made of a GaN thin film with a YAG: Ce yellow phosphor in 1997 by Nichia of Japan and then applying various light emitting chips and phosphors.

As a key element technology in a typical LED device, it is a high-efficiency, high-output chip and packaging technology. With the development of chip and module packaging technology, middle-low-brightness LEDs are being developed as high-brightness LEDs, ultimately becoming white LEDs for illumination.

A phosphor is a key material essential for the realization of white light because it is a substance that converts near-ultraviolet or blue light from an LED chip into an excitation source and turns it into visible light. Currently, we are concentrating on the development of high-quality emotional lighting capable of high color rendering and color temperature control by appropriately mixing green, yellow, and red phosphors along with high efficiency of illumination in advance of entering the general lighting market of white LED. Among them, the (acid) nitride phosphor in which all or a part of the oxygen atoms of the oxide material, which is generally industrialized at present, is replaced by a nitrogen atom, has a long wavelength excitation / emission characteristic and temperature / humidity stability due to strong covalent bonding and low electron affinity Because of its superiority, research on this issue has been concentrated around the world.

This is because in the long run, it is intended to replace the conventional oxide or sulfide phosphor with a nitride (oxynitride) phosphor in order to improve the durability of the illumination.

Particularly, a representative sialon (SiAlON) phosphor, which is a nitride (oxynitride), has a wide composition range and is a material which has recently been popularized as a material exhibiting a wide emission wavelength from green to red by control of composition. Typically, Japanese Patent Laid-Open Publication No. 2002-363554 discloses Ca _x Si _{12- (m + n)} Al _{m + n} O _n N _16-n : Eu _y- based phosphors whose emission peaks are in the range of 560 to 590 nm by pressure sintering. Since the proposal, many studies have been conducted to optimize the composition range such as rare earth content (Japanese Patent Laid-Open No. 2003-336059) or to optimize the manufacturing conditions (Japanese Patent Laid-Open No. 2005-8793).

Generally, a high-temperature process is required to synthesize a nitride phosphor having a high luminance. Particularly, since most of the nitride is covalently bonded to the oxide, it is known that diffusion as a mass transfer mechanism for synthesizing phosphors is kinetically disadvantageous even through a high temperature process. Therefore, a small amount of a sintering auxiliary agent is added to produce a eutectic liquid phase, and the material is promoted by a " dissolution-re-precipitation " mechanism to synthesize the phosphor. In this case, upon cooling after the high-temperature synthesis step, the phosphor particles synthesized by the amorphous grain boundary phase remaining between the grains are obtained in the form of a mass having strength by the sintering effect. (A) and (b) of FIG. 1 are an example of the photograph which image | photographed the normal nitride mass sintered compact, and generally volume shrinkage of about 65 to 75% arises.

Therefore, in order to produce a phosphor powder of a suitable size, a pulverization step is necessary as a post-treatment step.

When the average particle size is less than 1 micron, the emitted light is excessively scattered. When the particle size is large, it is difficult to uniformly disperse the phosphor in the resin in the packaging process, And color unevenness may be caused. Therefore, the average particle diameter of the phosphor is preferably 1 to 20 microns, more preferably 1 to 10 microns.

Therefore, the sintered phosphor must go through grinding and sieving processes for proper particle size. However, it has been pointed out that the generation of defects on the surface of the particles due to the pulverization of the phosphor particles, thereby lowering the luminance. This is because the light emission due to the excitation light radiates in the form of light rays from the inside and the outside of the phosphor particles, so that the surface defects generated by the pulverization treatment have a great influence on the fluorescence property and deteriorate the light emitting property. Therefore, the pulverizing process of the sintered phosphor necessarily has a close relationship with the luminescent characteristics of the phosphor.

In order to solve these problems, Japanese Unexamined Patent Publication (Kokai) No. 2005-8794 proposes a method of introducing a heat treatment process to heal surface defects after crushing, Japanese Unexamined Patent Publication No. 2005-255885 discloses a non- And a method of producing a phosphor without grinding by applying a post-acid cleaning process.

On the other hand, Japanese Patent Application Laid-Open No. 2007-57133 proposes a method of replacing a part of the source of an alkaline earth metal ion with a fluoride such as CaF2 to function as a flux, thereby suppressing sintering between particles and producing? -Sialon in which fluorine is dissolved in the crystal lattice And the like. The above patent reports that sialon can be easily made into fine particles by pulverization to a degree of decomposition, and control of the particle size range required as a phosphor is facilitated.

However, there is a lack of research on a method for producing nitride phosphors capable of pulverizing a low-energy powder and exhibiting a relatively uniform particle size and exhibiting a high luminance. In addition, sialon phosphors are generally produced in an acicular (or columnar) particle shape having a length ratio of " length / diameter " greater than 1. In order to improve the paving performance by mixing with a resin, It is desirable to develop a particle having a minimized shape or length ratio.

In order to solve the above problems of the prior art, the present invention provides a nitride phosphor capable of controlling the shape, size and surface defects of particles even by low energy grinding after synthesis

It is an object to provide a method.

In order to achieve the above technical problem, the present invention, M1 _x M2 _y Si _12-mn Al _{m + n} O _n N _16-n (M1 is at least one element selected from the group consisting of Li, Mg, Ca and Y, M2 is at least one element selected from the group consisting of Ce, Pr, Eu, Tb, Yb and Er, and is represented by 1.0 ≦ m ≦ 2.5, m = 2n, 0.02 ≦ y ≦ 0.15, m = 2x + 3y) A method for producing a SiAlON phosphor, comprising the steps of: preparing a starting material comprising a compound of silicon nitride, aluminum nitride, the M1, M2 metal in a predetermined ratio; Mixing 5-10% by weight of non-metal fluoride or non-metal chloride with a weight ratio of the starting material composition; And firing the mixture provides a method for producing α-SiAlON phosphor comprising the step of synthesizing α-SiAlON.

In the present invention, the fluoride and chloride are preferably included in the starting material composition 5 to 8% by weight. More preferably, the fluoride and chloride may be included in the starting material composition in a weight ratio of 5 to 7 wt%.

The present invention may further comprise the step of producing a phosphor powder by low energy grinding the synthesized α-SiAlON. The low energy pulverization herein refers to a pulverization process in which a defect does not occur on the particle surface. This is referred to as induced grinding, which is characterized in that the grinding is completed in a very short time. In this case, the phosphor powder may have a single peak in particle size distribution.

In the present invention, the non-metal fluoride is NH ₄ F, the non-metal chloride is preferably NH ₄ Cl.

In the present invention, M1 is preferably Ca.

According to the present invention, it is possible to provide a method for producing a nitride phosphor whose particle shape, size and surface defects can be controlled even by low energy grinding after synthesis of α sialon. In addition, the present invention can provide a process for synthesizing α sialon which is most suitable in terms of resin molding process and luminance uniformity.

1 (a) and 1 (b) are photographs of ordinary nitride block sintered bodies.
Figure 2 is a graph showing the results of XRD analysis of a flux-free conventional α-SiAlON phosphor powder.
3 is a photograph observed by electron microscopy after pulverizing the phosphor synthesized in a flux-free composition.
FIG. 4 is a graph showing a change in particle size distribution according to planetary milling time of phosphors milled by planetary milling after inducing milling of the phosphor of FIG. 3.
FIG. 5 is a photograph of a phosphor synthesized according to the presence or absence of NH 4 Cl according to an embodiment of the present invention after low energy-induced pulverization and observed with an electron microscope. FIG.
FIG. 6 is a graph illustrating measured PL characteristics of each phosphor powder of FIG. 5.
7 is a graph showing an XRD analysis result of each phosphor powder of FIG. 5.
FIG. 8 is a photograph of a phosphor synthesized according to the presence or absence of NH 4 F according to an embodiment of the present invention and observed with an electron microscope after low energy-induced crushing.
FIG. 9 is a graph illustrating measured PL characteristics of each phosphor powder of FIG. 8.
FIG. 10 is a graph showing an XRD analysis result of each phosphor powder of FIG. 8.
11 is a graph showing the results of measuring particle size distribution of the phosphor powders of FIGS. 5 and 8 after low energy-induced grinding.
FIG. 12 is a graph showing the PL characteristics of low-pulverized flux-free compositions, oil-milled specimens of flux-free compositions, and 6 wt% of NH 4 Cl and NH 4 F added as fluxes.
FIG. 13 is a graph showing an estimated composition of a sialon phosphor prepared in an embodiment of the present invention. FIG.
In the present invention, the content of NH 4 Cl, NH 4 F is set in consideration of both the uniform particle size and brightness. As will be described later, according to the present invention, the flux content has an optimized range in brightness characteristics. In the illustrated embodiment, the optimum point of the luminance characteristic is around 6% by weight, and deterioration of the luminance characteristic occurs when the flux content is increased or decreased. On the other hand, the flux content of 4 wt% or less increases the volume fraction of coarse particles and fine particles and causes a size variation among the phosphor particles. This is negative in terms of resin molding process and luminance uniformity. In addition, flux addition in excess of 8 wt% provides good particle size but causes a sharp decrease in luminance. Therefore, the preferred flux content in the present invention is 5 to 10 wt%, more preferably 5 to 8 wt%, and still more preferably 5 to 7 wt%.
Hereinafter, the present invention will be described in detail by explaining preferred embodiments of the present invention.

The composition of the? Sialon phosphors prepared in the present invention is generally expressed as follows.

Here, M1 is at least one element selected from the group consisting of Li, Mg, Ca and Y, and M2 is at least one element selected from the group consisting of Ce, Pr, Eu, Tb, Yb and Er. The composition of the host crystals and the concentration of the active ions satisfy the conditions of 1.0? M? 2.5, m = 2n, 0.02? Y? 0.15, and m = 2x + 3y.

The present invention is characterized by using an appropriate amount of flux (flux) of a nonmetal fluoride or chloride in the synthesis of the α sialon phosphor. The use of metallic elements in the flux is undesirable because it may affect the composition of the final result. Preferably the fluoride or chloride is NH4Cl, NH4F.

In the present invention, the content of NH 4 Cl, NH 4 F is set in consideration of both the uniform particle size and brightness. As will be described later, according to the present invention, the flux content has an optimized range in brightness characteristics. In the illustrated embodiment, the optimum point of the luminance characteristic is around 6% by weight, and deterioration of the luminance characteristic occurs when the flux content is increased or decreased. On the other hand, the flux content of less than 4% by weight increases the volume fraction of the coarse and fine particles and causes a size deviation between the phosphor particles. This is negative in view of the resin molding process and the luminance uniformity. Flux additions in excess of 8 wt% also provide good particle size but lead to a sharp decrease in brightness. Therefore, the preferred flux content in the present invention is 5 to 10 wt%, more preferably 5 to 8 wt%, even more preferably 5 to 7 wt%.

Hereinafter, the present invention will be described in detail by explaining preferred embodiments of the present invention.

Si3N4, AlN, CaCO3 and Eu2O3 powders are mixed as starting materials to synthesize α-SiAlON. The raw powder is weighed by the molar ratio. In the present embodiment, the flux is determined based on the composition determined by x = 0.895, y = 0.07, m = 2, n = 1 in the α-SiAlON compositional formula expressed as CaxEuySi12-m-nAlm + nOnN16-n. The phosphors were synthesized and evaluated for the composition added 0-10 wt% (Table 1). Two types of fluxes, NH4Cl and NH4F, were investigated that influence particle shape and block strength. In the wet process, silicon nitride balls and nylon containers were used, and industrial ethanol was used as the solvent, and planetary milling was performed for 4 hours, followed by wet mixing. Thereafter, the mixed powder obtained by drying using a rotary dryer is used for storage and firing in a vacuum desiccant after putting a sieve (# 325) into a plastic pack. In the dry process, the mixture was mixed using a household food mixer, and the obtained mixed powder was used for storage and firing in a vacuum desiccant through a sieving process. After mixing a certain amount of the mixed powder in the BN container by its own load by free fall, it was synthesized at high temperature under a nitrogen gas atmosphere. At high temperature synthesis, pressurized atmosphere is developed to 0.1 ~ 0.9MPa pressure. The synthesized phosphor was subjected to agate milling, which is a low energy pulverization process. Particularly, in the case of strong aggregates synthesized in the form of mass, fine phosphor was pulverized by planetary milling, which is a high energy pulverization process. As a planetary milling device, a stainless steel vessel lined with silicon nitride (Si3N4) ceramics and a silicon nitride ball with a diameter of 5 mm were used. Distilled water was used as the solvent and milled for 1 to 12 hours at a rate of 300 r / min.

Synthesized phosphor powder was analyzed by XRD, observation of shape and size by scanning electron microscope, particle size distribution measurement by particle size analyzer (Beckman coulter LS-13320 PSA) and PL measuring equipment (excitation 200W Xe lamp by PSI). The luminescence property was evaluated by.

FIG. 2 is a graph showing the results of XRD analysis of α-SiAlON phosphor powder synthesized in a flux-free composition. The peak shown in FIG. 2 coincides with the pattern of α-Si3N4 of JCPDS card # 41-0360, except that the position of the peak shifted in the low angle direction of 2θ due to an increase in lattice constant by solid solution of Ca, Al, and O. Can be. As can be seen in Figure 2, a single phase phosphor in which no phase other than α-SiAlON was observed was synthesized.

3 is a photograph observed by electron microscopy after pulverizing the phosphor synthesized in a flux-free composition. Depending on the strength and time of the induced grinding, strong aggregates of around 100 μm are observed, and magnification of the aggregates shows that they are composed of rod-like grains inherent in the silicon nitride system of several micrometers in size. have.

Phosphor pulverization was induced in the low energy process of several tens to hundreds of micrometers, and finally pulverized to several micrometers by planetary milling of the high energy process. As a planetary milling device, a stainless steel vessel lined with silicon nitride (Si3N4) ceramics and a silicon nitride ball with a diameter of 5 mm were used. Distilled water was used as the solvent and milled for 1 to 12 hours at a rate of 300 r / min. After stopping the milling machine for each time, the solution was collected and subjected to particle size analysis. The results are shown in FIG. 4. Referring to FIG. 4, the median diameter was reduced to about 8 μm by one hour milling, and decreased to about 4 μm by two hour milling, and then the particle size was linear to the size of 2 μm with increasing milling time. Slightly decreased.

5 is an electron microscope after low energy-induced pulverization of a phosphor composite having a flux-free composition (a) and NH 4 Cl added with 2, 4, 6, 8, 10 wt%, respectively (b, c, d, e, f) The photograph was observed. As the amount of flux increased, grinding was possible with less and less force during induction grinding.In the case of NH4Cl addition, 0 ~ 4wt% composition (a, b, c) decreased the aspect ratio with increasing flux, but the silicon nitride system It has its own rod-like grains. On the other hand, the NH 4 Cl addition amount of 6 ~ 10wt% composition (d, e, f) forms the granule (equiaxed grain) shows a distinct appearance from the silicon nitride inherent acicular particles. In addition, in the case of the composition of the flux of 6-10 wt% added showing the granular particles, it can be seen that the size of the unit aggregate composed of the granular particles increases with increasing amount of the flux.

Fig. 6 is a diagram showing the PL characteristics of each obtained phosphor powder. The maximum PL strength is measured when the composition of NH4Cl is added at 6wt%, and the PL property decreases as the amount added or decreased. In the case of 10 wt% addition, a marked drop in properties is observed. However, in any case, the PL strength was reduced compared to the flux-free composition. As shown in FIG. 5, since the aggregate size of the flux-free composition was the largest, the activator content per unit volume of the phosphor powder was large. The reason for this is that the light loss due to scattering is small. However, such coarse phosphor powder is not preferable in terms of resin molding process and luminance uniformity. On the other hand, it can be seen that the dominant wave length (DWL) of each composition shifts in the short wavelength direction as the amount of flux added increases (Fig. 6 (b)).

As shown in FIG. 6 (b), XRD analysis was performed to identify a phenomenon in which the DWL shifts in the short wavelength direction, and the results are shown in FIG. 7. Silicone powder was added in a weight ratio of 10: 1 as a standard for each phosphor powder sample. It can be seen that the α-SiAlON peak shifts in the direction of increasing 2θ (right) as the amount of NH 4 Cl is increased. In other words, as the amount of NH 4 Cl added increases, the transition to a structure closer to α-Si 3 N 4 means that the value of (m, n) indicating the solubility of α-SiAlON decreases. In general, it is known that in α-SiAlON, light emission shifts in the long wavelength direction as the value of the solid solution (m, n) increases. As measured in FIG. 6 (b), the light emission shifts in the short wavelength direction as the amount of flux added increases. One is because the high doses (m, n) were reduced as shown in FIG.

FIG. 8 shows the phosphor composite of the flux-free composition (a) and the composition (b, c, d, e, f) to which 2, 4, 6, 8, and 10 wt% are added, respectively, in an electron microscope It is photograph photographed by. As the amount of flux increased, low-energy processing was performed, which was possible to grind with less and less force during the induced grinding, but relatively low-energy grinding was possible compared to the NH 4 Cl addition composition of FIG. 5. Even though the amount of NH4F added increased, the needle-shaped particle shape inherent in the silicon nitride system observed in the flux-free composition was maintained. Nevertheless, the aspect ratio of the particles varied with the amount of flux added, which was minimal when the 6wt% was added (Fig. 8 (d)).

PL characteristics of the phosphor powder of FIG. 8 were evaluated and shown in FIG. 9. The maximum PL intensity of NH4F-added composition was measured at the addition of 6wt%, indicating the optimum composition point in terms of optical properties, but the PL strength was reduced compared to the flux-free composition (Fig. 9 (a)). The PL strength of the flux-free composition was larger than that of the flux-added composition because the size of the aggregate of the flux-free composition was the largest as shown in FIG. 8, and the activator content per unit volume of the phosphor powder was large. This is because the losses due to spawning are small.

On the other hand, it can be seen that the dominant wave length (DWL) of each composition shifts in the short wavelength direction as the amount of flux is increased (Fig. 9 (b)). The PL phenomena and the shift of DWL with the increase of NH4F addition tended to be the same as the case of NH4Cl addition.

As shown in FIG. 9 (b), XRD analysis was performed to identify a phenomenon in which the DWL shifts in the short wavelength direction and the results are shown in FIG. 10. Silicone powder was added in a weight ratio of 10: 1 as a standard for each phosphor powder sample. It can be seen that the α-SiAlON peak shifts in the direction (right) where 2θ increases as the amount of NH 4 F added increases. In other words, as the amount of NH 4 F added increases, the transition to a structure closer to α-Si 3 N 4 means that the value of (m, n) indicating the solubility of α-SiAlON decreases. In general, it is known that in α-SiAlON, light emission shifts in the long wavelength direction as the value of the solubility (m, n) increases. As measured in FIG. 9 (b), the light emission shifts in the short wavelength direction as the amount of flux added increases. One is because the high doses (m, n) were reduced as shown in FIG. 10.

Flux-free compositions are synthesized in bulk and require high energy pulverization, whereas flux addition compositions are easier to pulverize as flux increases. As shown in FIGS. 6 and 8, the flux-added composition has a lower PL strength than the flux-free composition, which is not measured in the form of particles separated when measuring the PL property, but for aggregates having different sizes. Because it was evaluated. 11 is a result of measuring the particle size distribution after low energy-induced grinding for the composite of the composition to which NH4Cl (FIG. 11 (a)) and NH4F (FIG. 11 (b)) are added.

Referring to FIG. 11, a typical vial having coarse particle peaks having a high volume fraction of 50 microns to 100 microns for flux-free compositions and fine particle peaks having a lower volume fraction below 10 microns It can be seen that the modal distribution. As the flux content increases, the volume fraction of the coarse particle peaks decreases. For the addition of 2 to 4 wt%, the volume fraction of the coarse particles of several tens of microns still occupies a considerable portion, and the volume fraction of the fine particles less than one micron is considerable, indicating that there is a very large variation in the phosphor particle size. Can be. When 6 wt% is added, it can be seen that the volume fraction of the coarse particles and the volume fraction of the fine particles decrease significantly at the same time. In addition, both NH 4 Cl and NH 4 F completely converted to a single peak upon addition of 8 wt%. Accordingly, it can be seen from the above examples that from the viewpoint of particle size distribution, flux of about 5 wt% or more is preferably added. The median diameter of the 6 wt% addition composition corresponding to the point of maximum PL strength was measured to be about 4.7 μm for NH 4 Cl and about 6.2 μm for NH 4 F.

As mentioned in FIG. 3, the particle size of the induced pulverization of the flux-free composition includes coarse aggregates of about 100 μm. In fact, the high energy pulverization process is additionally required in order to apply the resin molding process during packaging. In addition, when the phosphor having such a high deviation is dispersed, local luminance unevenness may occur. However, when flux is added, it can be seen that a phosphor powder having an appropriate size distribution can be produced even though only induced grinding, which is a low energy process as shown in FIG. 11.

As can be seen in Figures 6 and 9, NH4Cl and NH4F in common, the maximum PL strength was measured at the addition of 6wt%. At this time, the median particle diameters of the phosphor particles (aggregates) were 4.7 µm and 6.2 µm, respectively (Fig. 11).

Since the medium particle diameter of the sample subjected to high energy pulverization by planetary milling for 2 hours after the low energy-induced pulverization of the flux-free composition was about 4 μm, the PL characteristics of the sample and 6 wt% of NH4Cl and NH4F were respectively added. Compared. As shown in FIG. 12, the PL strength was increased in the order of flux-free (oil milling 2 hours) <NH 4 Cl 6 wt% <NH 4 F 6 wt% <flux-free. Therefore, it can be seen that similar particle size distribution shows high luminance characteristics in the sample to which 6 wt% of flux is added. On the other hand, flux-free (induced pulverization) showed the highest brightness, but when applied to the LED device is unsuitable for the resin molding process, it will be understood by everyone that it can cause unevenness of the brightness characteristics.

Hereinafter, the difference in luminance characteristics will be described as follows. However, the following description is not intended to limit the present invention but is only one way of interpreting the present invention, and other interpretations may be possible.

13 is a graph showing the estimated composition of the sialon phosphor prepared in the embodiment of the present invention. The estimated composition is a value calculated by the Rutten equation below from the lattice constant obtained from the XRD data.

Referring to FIG. 13, the composition originally designed by the stoichiometric ratio of the raw material powder was m = 2, but in the case of flux-free, m = 1.57. This is understood because sialon theoretically completely crystallizes without the grain boundary amorphous phase, but in reality the compositional variation occurs due to the residual grain boundary phase. On the other hand, when the flux is added, it can be seen that the m value decreases with the increase in the flux addition amount. The decrease in the m value means that the number of Al substituting Si decreases. It means decreasing. This reduction in high capacity will act as a cause of the decrease in luminance in terms of PL characteristics. On the other hand, since the pulverization of the synthesized phosphor mass is facilitated by flux addition, defect introduction is reduced, which is considered to have a positive effect on the PL properties.

Claims (8)

Composition M1xM2ySi12-m-nAlm + nOnN16-n (M1 is at least one element selected from the group consisting of Li, Mg, Ca, and Y, and M2 is 1 selected from the group consisting of Ce, Pr, Eu, Tb, Yb and Er). In the method for producing an α-SiAlON phosphor represented by an element or more, and expressed by 1.0 ≦ m ≦ 2.5, m = 2n, 0.02 ≦ y ≦ 0.15, m = 2x + 3y),
Preparing a starting material comprising a compound of silicon nitride, aluminum nitride, M1, M2 metal according to the composition formula;
Mixing 5-8% by weight of nonmetal fluoride or nonmetal chlorides by weight with the starting material;
Calcining the starting material passed through the mixing step to synthesize α-SiAlON; And
A method of producing α-SiAlON phosphor comprising the step of pulverizing the synthesized α-SiAlON to produce a phosphor powder.
delete delete delete The method of claim 1,
The phosphor powder has a particle size distribution has a single peak, characterized in that the α-SiAlON phosphor production method.
The method of claim 1,
The non-metal fluoride is NH 4 F, characterized in that the production method of α-SiAlON phosphor.
The method of claim 1,
The non-metal chloride is a method for producing α-SiAlON phosphor, characterized in that NH4Cl.
The method of claim 1,
Wherein M1 is Ca. The method for producing an? -SiAlON phosphor according to claim 1,

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